#------------------------------------------------------------------------------
#$Date: 2024-10-06 09:25:44 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295157 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/33/7133321.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133321
loop_
_publ_author_name
'Katzer, Nicholas J.'
'Kaur, Mandeep'
'Sen, Asmita'
'Nimaiyar, Rupal'
'Autschbach, Jochen'
'Arnold, Polly L.'
'Hintermair, Ulrich'
_publ_section_title
;
 Tetraphenylpentalenide organolanthanide complexes.
;
_journal_issue                   72
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9749
_journal_page_last               9752
_journal_paper_doi               10.1039/d4cc02570a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C48 H62 K2 O8'
_chemical_formula_sum            'C48 H62 K2 O8'
_chemical_formula_weight         845.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-18 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.8280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.14420(10)
_cell_length_b                   13.06880(10)
_cell_length_c                   16.74600(10)
_cell_measurement_reflns_used    34332
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      79.6210
_cell_measurement_theta_min      4.1070
_cell_volume                     2334.47(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -26.00   8.00   0.50    0.05    --   47.94 -19.00-180.00   68
  2  ω    -25.00  34.00   0.50    0.05    --   47.94 -37.00 -60.00  118
  3  ω    -26.00   8.00   0.50    0.05    --   47.94 -19.00 -30.00   68
  4  ω    -26.00   8.00   0.50    0.05    --   47.94 -19.00 120.00   68
  5  ω     85.00 111.00   0.50    0.21    --  113.25 -82.00  57.53   52
  6  ω     57.00 111.00   0.50    0.21    --  113.25-125.00  60.00  108
  7  ω     48.00  80.00   0.50    0.21    --  113.25-125.00 -60.00   64
  8  ω     86.00 111.00   0.50    0.21    --  113.25-125.00 -60.00   50
  9  ω     44.00 125.00   0.50    0.21    --  113.25-143.00 -91.18  162
 10  ω     44.00  91.00   0.50    0.21    --  113.25-125.00-150.00   94
 11  ω     47.00 108.00   0.50    0.21    --  113.25-106.00 -22.31  122
 12  ω      0.00  80.00   0.50    0.05    --   47.94 -99.00-120.00  160
 13  ω     42.00  83.00   0.50    0.21    --  113.25 -94.00  30.00   82
 14  ω     75.00 105.00   0.50    0.21    --  113.25 -94.00  90.00   60
 15  ω     70.00 104.00   0.50    0.21    --  113.25 -94.00 120.00   68
 16  ω     68.00 103.00   0.50    0.21    --  113.25 -94.00 150.00   70
 17  ω     78.00 107.00   0.50    0.21    --  113.25-104.00  48.50   58
 18  ω     43.00  69.00   0.50    0.21    --  113.25 -94.00   0.00   52
 19  ω     71.00  97.00   0.50    0.21    --  113.25 -94.00 -90.00   52
 20  ω     77.00 103.00   0.50    0.21    --  113.25 -90.00-174.44   52
 21  ω     68.00 106.00   0.50    0.21    --  113.25 -94.00-180.00   76
 22  ω     42.00 106.00   0.50    0.21    --  113.25 -94.00-150.00  128
 23  ω     42.00  86.00   0.50    0.21    --  113.25 -94.00-120.00   88
 24  ω     89.00 115.00   0.50    0.21    --  113.25 -88.00  46.29   52
 25  ω     57.00  82.00   0.50    0.21    --  113.25 -88.00  46.29   50
 26  ω     43.00  73.00   0.50    0.21    --  113.25 -82.00  57.53   60
 27  ω    103.00 128.00   0.50    0.21    --  113.25 -86.00 170.86   50
 28  ω     42.00  71.00   0.50    0.21    --  113.25 -61.00  90.00   58
 29  ω     58.00 112.00   0.50    0.21    --  113.25 -77.00  90.00  108
 30  ω     98.00 132.00   0.50    0.21    --  113.25 -77.00 -90.00   68
 31  ω     84.00 111.00   0.50    0.21    --  113.25 -77.00 -60.00   54
 32  ω     53.00  79.00   0.50    0.21    --  113.25 -77.00 -60.00   52
 33  ω     42.00  88.00   0.50    0.21    --  113.25 -77.00 -90.00   92
 34  ω     43.00  75.00   0.50    0.21    --  113.25 -77.00-150.00   64
 35  ω     51.00  80.00   0.50    0.21    --  113.25 -77.00-180.00   58
 36  ω     78.00 125.00   0.50    0.21    --  113.25 -77.00-150.00   94
 37  ω    100.00 135.00   0.50    0.21    --  113.25 -76.00 -41.98   70
 38  ω    105.00 131.00   0.50    0.21    --  113.25 -77.00   0.00   52
 39  ω     42.00  67.00   0.50    0.21    --  113.25 -61.00 -90.00   50
 40  ω     43.00  70.00   0.50    0.21    --  113.25 -61.00 -30.00   54
 41  ω     43.00  69.00   0.50    0.21    --  113.25 -61.00-120.00   52
 42  ω     44.00  70.00   0.50    0.21    --  113.25 -77.00  30.00   52
 43  ω     42.00  71.00   0.50    0.21    --  113.25 -61.00  60.00   58
 44  ω     46.00  73.00   0.50    0.21    --  113.25 -62.00 107.82   54
 45  ω    100.00 171.00   0.50    0.21    --  113.25  15.00  30.00  142
 46  ω    124.00 168.00   0.50    0.21    --  113.25  61.00 150.00   88
 47  ω    118.00 145.00   0.50    0.21    --  113.25  61.00 120.00   54
 48  ω    150.00 178.00   0.50    0.21    --  113.25  61.00 120.00   56
 49  ω    118.00 145.00   0.50    0.21    --  113.25  77.00  60.00   54
 50  ω    108.00 175.00   0.50    0.21    --  113.25  61.00 -60.00  134
 51  ω    120.00 175.00   0.50    0.21    --  113.25  77.00 -90.00  110
 52  ω    107.00 143.00   0.50    0.21    --  113.25  61.00-120.00   72
 53  ω    146.00 175.00   0.50    0.21    --  113.25  77.00-150.00   58
 54  ω    145.00 170.00   0.50    0.21    --  113.25  61.00-120.00   50
 55  ω    105.00 173.00   0.50    0.21    --  113.25  45.00-150.00  136
 56  ω    101.00 135.00   0.50    0.21    --  113.25  30.00-150.00   68
 57  ω    112.00 172.00   0.50    0.21    --  113.25  15.00  60.00  120
 58  ω    103.00 152.00   0.50    0.21    --  113.25  30.00 150.00   98
 59  ω    111.00 137.00   0.50    0.21    --  113.25  61.00  90.00   52
 60  ω    140.00 166.00   0.50    0.21    --  113.25  61.00  90.00   52
 61  ω    106.00 146.00   0.50    0.21    --  113.25  15.00 -90.00   80
 62  ω    122.00 148.00   0.50    0.21    --  113.25  15.00-120.00   52
 63  ω    100.00 140.00   0.50    0.21    --  113.25  15.00 -60.00   80
 64  ω    103.00 178.00   0.50    0.21    --  113.25 111.00  87.37  150
 65  ω    133.00 159.00   0.50    0.21    --  113.25 125.00 150.00   52
 66  ω    126.00 163.00   0.50    0.21    --  113.25 125.00  90.00   74
 67  ω    122.00 154.00   0.50    0.21    --  113.25 125.00   0.00   64
 68  ω    108.00 158.00   0.50    0.21    --  113.25 125.00 -60.00  100
 69  ω    149.00 175.00   0.50    0.21    --  113.25 125.00-120.00   52
 70  ω    119.00 145.00   0.50    0.21    --  113.25 125.00-180.00   52
 71  ω    102.00 128.00   0.50    0.21    --  113.25 125.00-120.00   52
 72  ω    138.00 170.00   0.50    0.21    --  113.25 117.00 120.62   64
 73  ω    -71.00  16.00   0.50    0.05    --  -47.94  77.00   0.00  174
 74  ω    -42.00  25.00   0.50    0.05    --  -47.94  37.00 -90.00  134
 75  ω    -16.00  28.00   0.50    0.05    --  -47.94  19.00 -30.00   88
 76  ω    -42.00  25.00   0.50    0.05    --  -47.94  37.00 150.00  134
 77  ω    -16.00  28.00   0.50    0.05    --  -47.94  19.00 120.00   88
 78  ω    -16.00  28.00   0.50    0.05    --  -47.94  19.00   0.00   88
 79  ω    -16.00  28.00   0.50    0.05    --  -47.94  19.00  30.00   88
 80  ω    -53.00 -20.00   0.50    0.21    --  -91.75  45.00 150.00   66
 81  ω   -163.00 -97.00   0.50    0.21    --  -91.75 -52.00 -87.45  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0011411000
_diffrn_orient_matrix_UB_12      -0.1163938000
_diffrn_orient_matrix_UB_13      -0.0142589000
_diffrn_orient_matrix_UB_21      -0.0757053000
_diffrn_orient_matrix_UB_22      -0.0162816000
_diffrn_orient_matrix_UB_23      0.0627251000
_diffrn_orient_matrix_UB_31      -0.1229717000
_diffrn_orient_matrix_UB_32      0.0089150000
_diffrn_orient_matrix_UB_33      -0.0714467000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.078
_diffrn_reflns_theta_min         4.144
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.192
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.95a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'intense red'
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0047(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5064
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0501P)²+0.4437P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4747
_reflns_number_total             5064
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc02570a2.cif
_cod_data_source_block           pla23074_refinalized
_cod_depositor_comments
'Adding full bibliography for 7133320--7133330.cif.'
_cod_database_code               7133321
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K2 O8 C50 H70'
_chemical_oxdiff_usercomment     NJK-07-043
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.621
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C23-C22 \\sim C26-C25
 with sigma of 0.02
 O5-C22 \\sim O3-C25 \\sim O4-C26 \\sim O4-C23
 with sigma of 0.02
 O3-C21 \\sim O5-C21 \\sim O4-C24
 with sigma of 0.02
3. Others
 Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(O5)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=1-FVAR(1)
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(O3)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B), C25(H25A,H25B), C22(H22A,H22B), C26(H26A,
 H26B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C10(H10), C12(H12), C7(H7), C9(H9), C8(H8), C15(H15),
 C14(H14), C13(H13)
4.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C21(H21D,H21E,H21F), C21(H21A,H21B,H21C), C20(H20A,H20B,
 H20C), C17(H17A,H17B,H17C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.143
_oxdiff_exptl_absorpt_empirical_full_min 0.906
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.65597(2) 0.46789(2) 0.66991(2) 0.04479(11) Uani 1 1 d . . . . .
O2 O 0.77190(11) 0.60118(9) 0.79573(7) 0.0591(3) Uani 1 1 d . . . . .
O4 O 0.70389(11) 0.30457(9) 0.77984(7) 0.0607(3) Uani 1 1 d D . . . .
O1 O 0.91960(10) 0.47119(10) 0.72795(8) 0.0623(3) Uani 1 1 d . . . . .
C3 C 0.64753(9) 0.55888(8) 0.50294(6) 0.0279(2) Uani 1 1 d . . . . .
C4 C 0.51774(9) 0.55304(7) 0.50241(6) 0.0264(2) Uani 1 1 d . . . . .
C2 C 0.68645(10) 0.45740(8) 0.49664(7) 0.0299(2) Uani 1 1 d . . . . .
C1 C 0.59030(9) 0.38623(8) 0.49621(6) 0.0282(2) Uani 1 1 d . . . . .
C11 C 0.73713(10) 0.64304(8) 0.52436(7) 0.0318(2) Uani 1 1 d . . . . .
C5 C 0.61560(10) 0.27740(8) 0.51215(6) 0.0311(2) Uani 1 1 d . . . . .
C6 C 0.53993(11) 0.21394(9) 0.54503(7) 0.0357(2) Uani 1 1 d . . . . .
H6 H 0.467896 0.241763 0.556479 0.043 Uiso 1 1 calc R U . . .
C16 C 0.72440(11) 0.72344(9) 0.57654(7) 0.0395(3) Uani 1 1 d . . . . .
H16 H 0.651302 0.726971 0.594743 0.047 Uiso 1 1 calc R U . . .
C10 C 0.72265(11) 0.23144(10) 0.49847(8) 0.0423(3) Uani 1 1 d . . . . .
H10 H 0.776420 0.271655 0.476269 0.051 Uiso 1 1 calc R U . . .
C12 C 0.84656(11) 0.64278(11) 0.49825(9) 0.0447(3) Uani 1 1 d . . . . .
H12 H 0.858626 0.589975 0.462349 0.054 Uiso 1 1 calc R U . . .
C7 C 0.56867(13) 0.11105(9) 0.56112(9) 0.0464(3) Uani 1 1 d . . . . .
H7 H 0.514776 0.069473 0.582153 0.056 Uiso 1 1 calc R U . . .
C9 C 0.75133(13) 0.12958(11) 0.51648(10) 0.0523(3) Uani 1 1 d . . . . .
H9 H 0.825110 0.101512 0.507687 0.063 Uiso 1 1 calc R U . . .
C8 C 0.67400(14) 0.06810(10) 0.54712(10) 0.0541(4) Uani 1 1 d . . . . .
H8 H 0.692884 -0.002274 0.558341 0.065 Uiso 1 1 calc R U . . .
C15 C 0.81613(15) 0.79818(10) 0.60234(10) 0.0556(4) Uani 1 1 d . . . . .
H15 H 0.805285 0.851282 0.638373 0.067 Uiso 1 1 calc R U . . .
C14 C 0.92272(15) 0.79628(12) 0.57631(12) 0.0668(5) Uani 1 1 d . . . . .
H14 H 0.985151 0.847620 0.593968 0.080 Uiso 1 1 calc R U . . .
C13 C 0.93703(13) 0.71845(13) 0.52414(12) 0.0627(4) Uani 1 1 d . . . . .
H13 H 1.009939 0.716580 0.505635 0.075 Uiso 1 1 calc R U . . .
C24 C 0.79005(19) 0.23307(15) 0.76353(13) 0.0756(5) Uani 1 1 d D . . . .
H24A H 0.751845 0.199322 0.709923 0.113 Uiso 1 1 calc R U . . .
H24B H 0.811405 0.181666 0.808021 0.113 Uiso 1 1 calc R U . . .
H24C H 0.866283 0.268950 0.761403 0.113 Uiso 1 1 calc R U . . .
C19 C 0.90262(17) 0.58889(16) 0.83098(12) 0.0725(5) Uani 1 1 d . . . . .
H19A H 0.919089 0.532072 0.871820 0.087 Uiso 1 1 calc R U . . .
H19B H 0.938865 0.652200 0.860779 0.087 Uiso 1 1 calc R U . . .
C18 C 0.96258(16) 0.56650(17) 0.76462(14) 0.0741(5) Uani 1 1 d . . . . .
H18A H 0.941489 0.620912 0.721688 0.089 Uiso 1 1 calc R U . . .
H18B H 1.054828 0.564737 0.788750 0.089 Uiso 1 1 calc R U . . .
C21 C 0.35805(17) 0.44544(18) 0.71931(13) 0.0752(5) Uani 1 1 d D . . . .
H21D H 0.338437 0.497670 0.675444 0.113 Uiso 0.292(9) 1 calc R U P A 2
H21E H 0.313625 0.461131 0.760496 0.113 Uiso 0.292(9) 1 calc R U P A 2
H21F H 0.331558 0.378187 0.694581 0.113 Uiso 0.292(9) 1 calc R U P A 2
H21A H 0.368504 0.487881 0.769113 0.113 Uiso 0.708(9) 1 calc R U P A 1
H21B H 0.288631 0.397463 0.714165 0.113 Uiso 0.708(9) 1 calc R U P A 1
H21C H 0.339633 0.489314 0.669778 0.113 Uiso 0.708(9) 1 calc R U P A 1
C20 C 0.7088(2) 0.61768(18) 0.85668(13) 0.0815(6) Uani 1 1 d . . . . .
H20A H 0.618224 0.620831 0.829606 0.122 Uiso 1 1 calc R U . . .
H20B H 0.737042 0.682330 0.885678 0.122 Uiso 1 1 calc R U . . .
H20C H 0.727257 0.561314 0.896997 0.122 Uiso 1 1 calc R U . . .
C17 C 0.98477(18) 0.4386(2) 0.67134(14) 0.0946(8) Uani 1 1 d . . . . .
H17A H 0.948623 0.374223 0.645175 0.142 Uiso 1 1 calc R U . . .
H17B H 1.073420 0.428200 0.701450 0.142 Uiso 1 1 calc R U . . .
H17C H 0.977356 0.490908 0.628231 0.142 Uiso 1 1 calc R U . . .
O3 O 0.4851(4) 0.4445(6) 0.7578(4) 0.0506(16) Uani 0.292(9) 1 d D . P A 2
O5 O 0.46886(18) 0.3905(3) 0.72631(19) 0.0623(10) Uani 0.708(9) 1 d D . P A 1
C25 C 0.5206(9) 0.3687(9) 0.8207(6) 0.064(2) Uani 0.292(9) 1 d D . P A 2
H25A H 0.444865 0.342376 0.833373 0.076 Uiso 0.292(9) 1 calc R U P A 2
H25B H 0.575682 0.399862 0.872255 0.076 Uiso 0.292(9) 1 calc R U P A 2
C22 C 0.5028(3) 0.3240(4) 0.7959(2) 0.0583(8) Uani 0.708(9) 1 d D . P A 1
H22A H 0.427856 0.287327 0.801387 0.070 Uiso 0.708(9) 1 calc R U P A 1
H22B H 0.539285 0.363619 0.847587 0.070 Uiso 0.708(9) 1 calc R U P A 1
C26 C 0.5868(12) 0.2834(9) 0.7951(8) 0.079(4) Uani 0.292(9) 1 d D . P A 2
H26A H 0.601409 0.230145 0.838928 0.095 Uiso 0.292(9) 1 calc R U P A 2
H26B H 0.530103 0.253530 0.743605 0.095 Uiso 0.292(9) 1 calc R U P A 2
C23 C 0.5961(4) 0.2496(4) 0.7830(3) 0.0574(9) Uani 0.708(9) 1 d D . P A 1
H23A H 0.618168 0.199695 0.829418 0.069 Uiso 0.708(9) 1 calc R U P A 1
H23B H 0.560742 0.211752 0.730203 0.069 Uiso 0.708(9) 1 calc R U P A 1
H2 H 0.7718(14) 0.4383(11) 0.5016(9) 0.040(4) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0941
0 0 1 0.1432
0 -1 -1 0.0604
1 -1 1 0.0858
-1 -2 0 0.1057
0 1 1 0.1016
-2 1 -1 0.0900
-2 -1 -1 0.0786
1 -1 -1 0.0664
2 -1 1 0.0785
-1 -2 2 0.1112
0 2 -1 0.0902
-1 2 -2 0.0901
1 1 -1 0.0753
0 1 -2 0.0828
-2 -1 2 0.1280
2 1 -1 0.0630
0 -1 1 0.0994
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 K1 O4 91.23(3) . . ?
O2 K1 O1 60.93(4) . . ?
O2 K1 C3 110.01(3) . . ?
O2 K1 C4 118.82(3) . . ?
O2 K1 C4 145.85(3) . 3_666 ?
O2 K1 C2 127.30(3) . . ?
O2 K1 C1 154.35(3) . . ?
O4 K1 O1 78.52(4) . . ?
O4 K1 C3 150.37(3) . . ?
O4 K1 C4 148.98(3) . . ?
O4 K1 C4 121.23(3) . 3_666 ?
O4 K1 C2 123.38(3) . . ?
O4 K1 C1 108.56(3) . . ?
O1 K1 C3 93.63(3) . . ?
O1 K1 C4 130.91(3) . 3_666 ?
O1 K1 C4 121.32(3) . . ?
O1 K1 C2 86.33(3) . . ?
O1 K1 C1 106.20(3) . . ?
C3 K1 C2 27.00(3) . . ?
C4 K1 C3 45.76(3) 3_666 . ?
C4 K1 C3 27.83(3) . . ?
C4 K1 C4 27.81(4) 3_666 . ?
C4 K1 C2 44.59(3) . . ?
C4 K1 C2 44.70(3) 3_666 . ?
C1 K1 C3 45.89(3) . . ?
C1 K1 C4 46.03(3) . . ?
C1 K1 C4 28.07(3) . 3_666 ?
C1 K1 C2 27.30(3) . . ?
O3 K1 O2 84.52(18) . . ?
O3 K1 O4 65.61(11) . . ?
O3 K1 O1 129.37(11) . . ?
O3 K1 C3 134.61(8) . . ?
O3 K1 C4 107.18(8) . . ?
O3 K1 C2 143.11(14) . . ?
O3 K1 C1 118.12(16) . . ?
O5 K1 O2 101.93(10) . . ?
O5 K1 O4 60.15(5) . . ?
O5 K1 O1 135.56(5) . . ?
O5 K1 C3 130.33(5) . . ?
O5 K1 C4 87.35(7) . 3_666 ?
O5 K1 C4 103.00(5) . . ?
O5 K1 C2 128.84(9) . . ?
O5 K1 C1 102.07(9) . . ?
C19 O2 K1 116.53(10) . . ?
C19 O2 C20 112.57(14) . . ?
C20 O2 K1 115.34(12) . . ?
C24 O4 K1 112.96(11) . . ?
C24 O4 C26 127.6(5) . . ?
C26 O4 K1 105.0(5) . . ?
C23 O4 K1 114.5(2) . . ?
C23 O4 C24 107.6(2) . . ?
C18 O1 K1 110.67(10) . . ?
C18 O1 C17 112.44(17) . . ?
C17 O1 K1 116.77(11) . . ?
C4 C3 K1 75.37(6) . . ?
C4 C3 C11 130.81(9) . . ?
C2 C3 K1 76.73(6) . . ?
C2 C3 C4 106.20(9) . . ?
C2 C3 C11 121.64(9) . . ?
C11 C3 K1 103.53(6) . . ?
K1 C4 K1 152.19(4) 3_666 . ?
C3 C4 K1 76.79(6) . . ?
C3 C4 K1 112.23(6) . 3_666 ?
C3 C4 C1 143.71(9) . 3_666 ?
C4 C4 K1 76.50(7) 3_666 3_666 ?
C4 C4 K1 75.69(7) 3_666 . ?
C4 C4 C3 108.04(10) 3_666 . ?
C4 C4 C1 108.25(10) 3_666 3_666 ?
C1 C4 K1 113.15(6) 3_666 . ?
C1 C4 K1 75.89(5) 3_666 3_666 ?
K1 C2 H2 108.2(9) . . ?
C3 C2 K1 76.27(6) . . ?
C3 C2 C1 111.69(9) . . ?
C3 C2 H2 123.7(9) . . ?
C1 C2 K1 74.90(6) . . ?
C1 C2 H2 123.8(9) . . ?
C4 C1 K1 76.04(6) 3_666 . ?
C4 C1 C5 130.45(9) 3_666 . ?
C2 C1 K1 77.80(6) . . ?
C2 C1 C4 105.73(9) . 3_666 ?
C2 C1 C5 122.20(9) . . ?
C5 C1 K1 100.97(6) . . ?
C16 C11 C3 122.25(10) . . ?
C16 C11 C12 116.65(11) . . ?
C12 C11 C3 120.92(11) . . ?
C6 C5 C1 122.77(10) . . ?
C6 C5 C10 116.35(10) . . ?
C10 C5 C1 120.82(10) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 121.10(12) . . ?
C7 C6 H6 119.5 . . ?
C11 C16 H16 119.2 . . ?
C15 C16 C11 121.57(13) . . ?
C15 C16 H16 119.2 . . ?
C5 C10 H10 119.1 . . ?
C9 C10 C5 121.81(13) . . ?
C9 C10 H10 119.1 . . ?
C11 C12 H12 119.5 . . ?
C13 C12 C11 121.09(14) . . ?
C13 C12 H12 119.5 . . ?
C6 C7 H7 119.3 . . ?
C8 C7 C6 121.30(13) . . ?
C8 C7 H7 119.3 . . ?
C10 C9 H9 119.6 . . ?
C8 C9 C10 120.79(13) . . ?
C8 C9 H9 119.6 . . ?
C7 C8 C9 118.62(12) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
C16 C15 H15 119.6 . . ?
C14 C15 C16 120.84(15) . . ?
C14 C15 H15 119.6 . . ?
C15 C14 H14 120.6 . . ?
C15 C14 C13 118.78(13) . . ?
C13 C14 H14 120.6 . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.06(15) . . ?
C14 C13 H13 119.5 . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
O4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C19 H19A 109.6 . . ?
O2 C19 H19B 109.6 . . ?
O2 C19 C18 110.07(15) . . ?
H19A C19 H19B 108.2 . . ?
C18 C19 H19A 109.6 . . ?
C18 C19 H19B 109.6 . . ?
O1 C18 C19 109.33(15) . . ?
O1 C18 H18A 109.8 . . ?
O1 C18 H18B 109.8 . . ?
C19 C18 H18A 109.8 . . ?
C19 C18 H18B 109.8 . . ?
H18A C18 H18B 108.3 . . ?
H21D C21 H21E 109.5 . . ?
H21D C21 H21F 109.5 . . ?
H21E C21 H21F 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 C21 H21D 109.5 . . ?
O3 C21 H21E 109.5 . . ?
O3 C21 H21F 109.5 . . ?
O5 C21 H21A 109.5 . . ?
O5 C21 H21B 109.5 . . ?
O5 C21 H21C 109.5 . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C17 H17A 109.5 . . ?
O1 C17 H17B 109.5 . . ?
O1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C21 O3 K1 121.9(3) . . ?
C21 O3 C25 112.5(5) . . ?
C25 O3 K1 112.9(4) . . ?
C21 O5 K1 121.69(19) . . ?
C21 O5 C22 113.7(2) . . ?
C22 O5 K1 117.72(16) . . ?
O3 C25 H25A 109.3 . . ?
O3 C25 H25B 109.3 . . ?
O3 C25 C26 111.7(7) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
O5 C22 H22A 110.0 . . ?
O5 C22 H22B 110.0 . . ?
O5 C22 C23 108.3(3) . . ?
H22A C22 H22B 108.4 . . ?
C23 C22 H22A 110.0 . . ?
C23 C22 H22B 110.0 . . ?
O4 C26 C25 117.9(8) . . ?
O4 C26 H26A 107.8 . . ?
O4 C26 H26B 107.8 . . ?
C25 C26 H26A 107.8 . . ?
C25 C26 H26B 107.8 . . ?
H26A C26 H26B 107.2 . . ?
O4 C23 C22 108.2(3) . . ?
O4 C23 H23A 110.1 . . ?
O4 C23 H23B 110.1 . . ?
C22 C23 H23A 110.1 . . ?
C22 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O2 2.7507(12) . ?
K1 O4 2.7678(12) . ?
K1 O1 2.8151(11) . ?
K1 C3 3.0148(10) . ?
K1 C4 2.9858(10) 3_666 ?
K1 C4 2.9963(10) . ?
K1 C2 3.0206(11) . ?
K1 C1 2.9838(10) . ?
K1 O3 2.740(4) . ?
K1 O5 2.7207(19) . ?
O2 C19 1.414(2) . ?
O2 C20 1.414(2) . ?
O4 C24 1.422(2) . ?
O4 C26 1.428(11) . ?
O4 C23 1.414(4) . ?
O1 C18 1.410(2) . ?
O1 C17 1.416(2) . ?
C3 C4 1.4459(13) . ?
C3 C2 1.4087(15) . ?
C3 C11 1.4588(14) . ?
C4 C4 1.4375(19) 3_666 ?
C4 C1 1.4479(13) 3_666 ?
C2 C1 1.4173(14) . ?
C2 H2 0.963(15) . ?
C1 C5 1.4594(14) . ?
C11 C16 1.3997(17) . ?
C11 C12 1.4097(16) . ?
C5 C6 1.4039(16) . ?
C5 C10 1.4124(15) . ?
C6 H6 0.9500 . ?
C6 C7 1.3905(17) . ?
C16 H16 0.9500 . ?
C16 C15 1.3894(18) . ?
C10 H10 0.9500 . ?
C10 C9 1.3817(19) . ?
C12 H12 0.9500 . ?
C12 C13 1.3890(19) . ?
C7 H7 0.9500 . ?
C7 C8 1.381(2) . ?
C9 H9 0.9500 . ?
C9 C8 1.381(2) . ?
C8 H8 0.9500 . ?
C15 H15 0.9500 . ?
C15 C14 1.379(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.380(3) . ?
C13 H13 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C18 1.482(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C21 H21D 0.9800 . ?
C21 H21E 0.9800 . ?
C21 H21F 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 O3 1.375(4) . ?
C21 O5 1.403(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O3 C25 1.417(7) . ?
O5 C22 1.415(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.468(10) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.483(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 O2 C19 C18 40.5(2) . . . . ?
K1 O4 C26 C25 -51.7(10) . . . . ?
K1 O4 C23 C22 -50.9(3) . . . . ?
K1 O1 C18 C19 54.96(17) . . . . ?
K1 C3 C4 K1 -152.33(5) . . . 3_666 ?
K1 C3 C4 C4 -69.92(9) . . . 3_666 ?
K1 C3 C4 C1 111.27(15) . . . 3_666 ?
K1 C3 C2 C1 67.31(8) . . . . ?
K1 C3 C11 C16 -58.78(11) . . . . ?
K1 C3 C11 C12 116.26(10) . . . . ?
K1 C2 C1 C4 71.50(7) . . . 3_666 ?
K1 C2 C1 C5 -95.39(9) . . . . ?
K1 C1 C5 C6 71.02(10) . . . . ?
K1 C1 C5 C10 -106.01(10) . . . . ?
K1 O3 C25 C26 -34.9(9) . . . . ?
K1 O5 C22 C23 -45.1(3) . . . . ?
O2 C19 C18 O1 -65.0(2) . . . . ?
C3 C2 C1 K1 -68.17(8) . . . . ?
C3 C2 C1 C4 3.33(12) . . . 3_666 ?
C3 C2 C1 C5 -163.56(10) . . . . ?
C3 C11 C16 C15 174.20(11) . . . . ?
C3 C11 C12 C13 -174.70(12) . . . . ?
C4 C3 C2 K1 -70.20(7) . . . . ?
C4 C3 C2 C1 -2.89(12) . . . . ?
C4 C3 C11 C16 23.44(17) . . . . ?
C4 C3 C11 C12 -161.52(11) . . . . ?
C4 C1 C5 C6 -9.91(17) 3_666 . . . ?
C4 C1 C5 C10 173.06(11) 3_666 . . . ?
C2 C3 C4 K1 -81.16(8) . . . 3_666 ?
C2 C3 C4 K1 71.17(7) . . . . ?
C2 C3 C4 C4 1.25(13) . . . 3_666 ?
C2 C3 C4 C1 -177.56(13) . . . 3_666 ?
C2 C3 C11 C16 -141.37(11) . . . . ?
C2 C3 C11 C12 33.66(16) . . . . ?
C2 C1 C5 C6 153.42(10) . . . . ?
C2 C1 C5 C10 -23.61(16) . . . . ?
C1 C5 C6 C7 -178.54(10) . . . . ?
C1 C5 C10 C9 177.20(12) . . . . ?
C11 C3 C4 K1 -95.40(11) . . . . ?
C11 C3 C4 K1 112.27(11) . . . 3_666 ?
C11 C3 C4 C4 -165.32(11) . . . 3_666 ?
C11 C3 C4 C1 15.9(2) . . . 3_666 ?
C11 C3 C2 K1 97.88(9) . . . . ?
C11 C3 C2 C1 165.19(9) . . . . ?
C11 C16 C15 C14 0.8(2) . . . . ?
C11 C12 C13 C14 0.0(2) . . . . ?
C5 C6 C7 C8 1.46(19) . . . . ?
C5 C10 C9 C8 1.4(2) . . . . ?
C6 C5 C10 C9 -0.02(18) . . . . ?
C6 C7 C8 C9 0.0(2) . . . . ?
C16 C11 C12 C13 0.60(18) . . . . ?
C16 C15 C14 C13 -0.2(2) . . . . ?
C10 C5 C6 C7 -1.39(16) . . . . ?
C10 C9 C8 C7 -1.4(2) . . . . ?
C12 C11 C16 C15 -1.04(17) . . . . ?
C15 C14 C13 C12 -0.3(2) . . . . ?
C24 O4 C26 C25 172.6(6) . . . . ?
C24 O4 C23 C22 -177.3(2) . . . . ?
C21 O3 C25 C26 107.9(9) . . . . ?
C21 O5 C22 C23 163.4(4) . . . . ?
C20 O2 C19 C18 177.04(17) . . . . ?
C17 O1 C18 C19 -172.46(16) . . . . ?
O3 C25 C26 O4 63.3(12) . . . . ?
O5 C22 C23 O4 62.7(4) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0003 -0.0016 -0.9995 0.0144 -0.0626 0.0714
0.0003 0.0016 0.9995 -0.0144 0.0626 -0.0714
-0.0020 -1.0009 -0.9970 0.1307 -0.0461 0.0626
0.9986 -0.9970 1.0002 0.1029 0.0034 -0.2031
-1.0033 -1.9992 0.0068 0.2314 0.1089 0.1051
0.0020 1.0009 0.9970 -0.1307 0.0461 -0.0626
-1.9985 0.9963 -0.9984 -0.1040 0.0725 0.3260
-2.0019 -1.0022 -0.9934 0.1285 0.1056 0.3082
0.9980 -1.0002 -0.9988 0.1318 -0.1219 -0.0603
1.9985 -0.9963 0.9984 0.1040 -0.0725 -0.3260
-1.0027 -1.9959 2.0058 0.2026 0.2342 -0.0378
0.0031 1.9969 -1.0045 -0.2181 -0.0958 0.0892
-0.9972 1.9946 -2.0022 -0.2047 -0.0826 0.2835
1.0013 0.9983 -1.0038 -0.1007 -0.1550 -0.0425
0.0011 0.9960 -2.0015 -0.0874 -0.1418 0.1517
-2.0010 -0.9973 2.0051 0.0852 0.2935 0.0939
2.0013 0.9989 -1.0056 -0.0996 -0.2308 -0.1654
-0.0014 -0.9976 1.0020 0.1018 0.0792 -0.0803
